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Structural and optical properties of pure SnO2 and V2O5/SnO2 nanocomposite

thin films for gas sensing application

Article  in  Journal of Materials Science Materials in Electronics · August 2020

DOI: 10.1007/s10854-020-04110-2

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Journal of Materials Science: Materials in Electronics
https://doi.org/10.1007/s10854-020-04110-2

Structural and optical properties of pure ­SnO2 and ­V2O5/SnO2

nanocomposite thin films for gas sensing application
V. Janakiraman1 · V. Tamilnayagam2 · R. S. Sundararajan1 · S. Suresh3   · C. S. Biju4

Received: 16 May 2020 / Accepted: 25 July 2020

© Springer Science+Business Media, LLC, part of Springer Nature 2020

Abstract
In this study, pure S­ nO2 and V
­ 2O5/SnO2 nanocomposite thin film N ­ H3 sensors with varying V
­ 2O5 contents were successfully
prepared by spray pyrolysis method. The prepared thin films were characterized by X-ray diffraction, Field emission scanning
electron microscopy, Energy dispersive X-ray spectroscopy, Fourier-transform infrared spectroscopy, stylus profilometry and
Ultra violet–Visible and transmittance spectroscopies. ­NH3 gas sensing property was also studied. XRD results suggested
that all the thin films exhibited a tetragonal rutile crystal structure, while the average crystallite size increases with ­V2O5
content. FESEM images of the thin films showed the presence of both nano and micro-sized grains in the range ~ 53–194 nm.
EDX spectra confirmed the inclusion of V ­ 2O5 into the S
­ nO2 matrix. The vibrational bands associated with the thin films
were verified from the FTIR spectra. Thickness measurements revealed that the thickness increases with V ­ 2O5 content.
Change in transparency and bandgap narrowing were also noticed from the transmittance and UV–Vis spectra. N ­ H3 gas
sensing measurements suggested that the transient resistance of V ­ 2O5/SnO2 thin film was lower than pure S ­ nO2. Further, in
the operating temperature 300 °C and 100 ppm NH3 gas, the sensor response of ­V2O5/ ­SnO2 thin film (99.13) is found to
be higher than pure S ­ nO2 thin film (92.34). Also, the response and recovery times of pure S­ nO2 thin film (30 and 44 s) are
lower than V ­ 2O5/SnO2 thin film (39 and 180 s). These results indicate that ­V2O5/SnO2 thin film could serve as a suitable
material for ­NH3 gas sensing application.

1 Introduction and consequently vomit and headache occurs. Therefore

Ammonia ­(NH3) is considered as one of the key precursors
to synthesize various materials in chemical industries [1].
It is a colourless gas which could stimulate eye and nose,
* V. Janakiraman
v.raman.in@gmail.com
* S. Suresh
sureshthanjai2003@gmail.com
* C. S. Biju
zliffyplanet@gmail.com
1
PG & Research Department of Physics, Government
Arts College (Autonomous) (Affiliated to Bharathidasan
University), Kumbakonam, Tamil Nadu 612002, India
2
Department of Physics, A.P.A. College of Arts & Culture,
Palani, Dindigul, Tamil Nadu, India
3
Departments of Physics, Saveetha Engineering College
(Autonomous), Thandalam, Chennai, Tamil Nadu 602105,
India
4
Department of Physics, Malankara Catholic College,
Mariagiri, Kaliakkavilai, Tamil Nadu 629153, India
an attractive method to sense the presence of ­NH3 in the
atmosphere is much essential in the field of environmen-
tal measurement and control. Semiconductor-based sensors
have been extensively investigated to detect gas components
even at low level [2]. In particular, tin oxide (­ SnO2)-based
thin films are much appropriate for gas sensor development
[3–5]. Various strategies such as doping with Eu [6], La
[7], Ce [8], etc., have shown excellent response and recov-
ery even at low parts per million (ppm) concentration. Over
the years, formation of composites with S ­ nO2 has gained
increased attention to develop high sensitive sensors. In this
view, composites such as ­WO3/SnO2 [9], Au@TiO2/SnO2
[10] and ­Sm2O3/SnO2 [11] have been prepared and shown
enhanced response for various volatile gases. It has been
demonstrated that efficient charge transfer in the composite
is a key to ensure high response [12]. Indeed, N ­ H3 sensing
performance using ­SnO2-based composites is still limited.
Various ­SnO2-based nanocomposites have been explored as
a potential ­NH3 gas sensor due to their unique interface and
synergetic effects [13–15]. Materials such as multi-walled
carbon nanotube (MWCNT), Pd/reduced graphene oxide

13
Vol.:(0123456789)

(RGO) and S ­ nS2 have been effectively coupled with S
­ nO2 to
improve the sensing parameters (sensor response, response
time and recovery time) [13–15]. However, N ­ H3 gas sen-
sors fabricated using these materials showcased limited sen-
sor response as well as slow response and recovery times.
Therefore a reliable and unique coupling material which
promotes excellent ­NH3 gas sensor response is highly desir-
able. Bare ­V2O5 is regarded as a suitable sensor material
which presents significant improvement in sensor response
by reducing the resistance of the material, upon exposure to
­NH3 gas [16]. Coupling of V ­ 2O5 with S­ nO2 has also shown
tremendous sensor response towards various volatile gases
[17]. It is well known that ­SnO2-based nanocomposites can
be prepared in the form of powder as well as thin film. Com-
pared to powder form, S ­ nO2-based thin films prepared by
micro-fabrication processes are more compatible for direct
sensor application [18]. So for ­V2O5/SnO2, nanocomposites
have been prepared by molecule-based CVD [19], gas phase
base [20] and solid phase sol–gel methods [21]. Further,
­V2O5/SnO2 nanocomposite has displayed a red shift in pho-
toconductance [19], very good cycling stability for lithium-
ion battery [20] and better gas response towards 50 ppm of
benzene, toluene, ethylene and xylol (BTEX) gases at an
operating temperature of 210 °C [21]. To the best of our
knowledge, there have been no reports on the preparation
of ­V2O5/SnO2 nanocomposite thin film by spray pyrolysis
method and its ­NH3 gas sensing property. These affirma-
tions motivated us to carry out the ­NH3 gas sensor study for
pure ­SnO2 and ­V2O5/SnO2 nanocomposite thin films. The
aim of this work was to prepare ­V2O5/SnO2 nanocompos-
ite thin films with varying weight ratios of V ­ 2O5 content
by spray pyrolysis method. The deposited thin films were
characterized by X-ray diffraction (XRD), Field emission
scanning electron microscopy (FESEM), Energy disper-
sive X-ray (EDX) spectroscopy, Fourier-transform infrared
(FTIR) spectroscopy, stylus profilometry, Ultraviolet–Visi-
ble (UV–Vis) and transmittance spectroscopies, respectively.
­NH3 gas sensing measurement was carried out to observe the
change in transient resistance as a function of time.
2 Experimental techniques
2.1 Deposition of pure ­SnO2 and ­V2O5/SnO2 thin
films
Vanadium(V) oxide (­ V2O5, 99.95%) and Tin(II) chloride
dihydrate ­( SnCl 2·2H 2O, 99.99%) were purchased from
Sigma Aldrich, Mumbai. Thin films were deposited on
glass substrates by spray pyrolysis method. Prior to thin
film preparation, the substrates were cleaned in an ultra-
sonic bath with deionized (D.I) water and stored in a dried
box. To prepare pure ­SnO2 thin film (SV0), ­SnCl2·2H2O was
13
Journal of Materials Science: Materials in Electronics
dissolved in D.I water under constant stirring at room tem-
perature. The prepared solution was continuously sprayed on
the glass substrate kept on a hot plate, which was maintained
at 400 °C in air. The distance between the substrate surface
and spray nozzle was fixed at 20 cm and the spray rate was
maintained at 1.8 mL/min. To prepare V ­ 2O5/SnO2 nanocom-
posite thin films with varying weight ratios of V ­ 2O5 and
­SnO2, suitable quantities of V ­ 2O5 powders were dispersed
into the above solution under constant stirring. Other experi-
mental conditions were kept quite similar to the preparation
of SV0 thin film. The V­ 2O5/SnO2 nanocomposite thin films
were prepared in the weight ratios (­ V2O5:SnO2) 2:98, 4:96,
6:94, 8:92 and 10:90 and labelled as SV1, SV2, SV3, SV4
and SV5, respectively.
2.2 Characterizations
Crystal structure analysis was carried out using a XRD
(Rigaku III) with Cu K radiation in the range 10–80° and
scan speed of 1° m ­ in−1. The surface morphology, size and
presence of elements were examined by means of a FESEM
(Hitachi S-4800 model) equipped with an EDX (TESCAN
SEM-VEGA III) spectroscope. The vibrational bands related
to the thin films were analysed with the assistance of a FTIR
(Bruker Model IFS 66V Spectrophotometer), which was
recorded in the wavelength range 3000−400  cm−1. The
thickness of the thin films was measured by contact method
with help of a stylus profilometer (Surftest SJ − 301). The
transmittance and absorption spectra were acquired using
a UV–Vis spectrophotometer (VARIAN CARY 5E) in the
wavelength range 300–1100 nm.
2.3 Gas sensing measurements
Thin films of size (1 × 1 cm) were used to measure the
change in transient resistance as a function of time, when
exposed to N­ H3 gas. Silver paste contacts were made at the
ends of the thin film sensors and the terminals were con-
nected to the probes of a source measure meter (Keithley
6517B). Constant concentration (100 ppm) of ­NH3 gas was
injected into the test chamber, while the relative humidity
was kept at 60% in the chamber using a digital humidity
controller (Humitherm, India). A constant temperature of
300 °C was maintained to measure the change in transient
resistance of the thin films. At this operating temperature
(300 °C), the rate of adsorption and desorption of ­NH3 gas
increases and makes the sensor response to reach its maxi-
mum [22]. Response time is the time taken by the sensor to
attain 90% of the total change in resistance in the presence
of ­NH3 gas, while the time taken by the sensor to recover
90% of the baseline signal is called recovery time [22]. The
schematic illustrations of sensor platform and sensor setup
are presented in the Fig. 1a and b.
Journal of Materials Science: Materials in Electronics
Fig. 1  Schematic illustrations of
a sensor platform and b sensor
setup
3 Results and discussion
3.1 XRD analysis
Figure 2 shows the XRD patterns of the thin films SV0–SV5.
All the thin films exhibit several diffraction peaks corre-
sponding to the planes (110), (101), (200), (211), (220),
(310) and (301). These diffraction peaks match well with the
tetragonal rutile phase of S
­ nO2 (JCPDS Card No. 01-0657)
[23]. The absence of ­V2O5 phase peaks indicate that rutile
phase of ­SnO2 is unaffected due to the inclusion of ­V2O5 into
the ­SnO2 matrix. However, an additional peak belonging to
the plane (110) is identified in the thin films from SV0 to
SV4, which is absent in SV5. This plane can be indexed to
the SnO phase of tin oxide (JCPDS Card No. 06-0395) [24].
The observed diffraction peaks are also sharp and strong,
which suggest the high crystal quality of the thin films. The
average crystallite size of the thin films could be calculated
using the Scherrer formula (Eq. 1) [25].
k𝜆
D = (1)
𝛽 cos 𝜃
where k is a constant (0.9), λ is the wave length of X-ray
(0.154 nm), β is the full width at half maximum (FWHM)
of the diffraction peaks (radian) and θ is the Bragg’s angle
(radian). The calculated average crystallite size of the
thin films SV0–SV5 are 51 nm, 70 nm, 79.27 nm, 82 nm,
83 nm and 93.23 nm, respectively. This result indicates that,
increase of V­ 2O5 content can effectively increase the aver-
age crystallite size of the thin films. It has been reported
that, upon increasing the content of the metal oxide-based
nanocomposite thin films, the average crystallite size also
increases [26]. However, a decrease in crystallite size has
also been reported in ZnO/SnO 2 nanocomposite [27].
Indeed, the growth of average crystallite size with increase
in ­V2O5 content is related to the increase in film thickness,
as evident from the thickness measurement study.
3.2 FESEM and EDX analyses
Figure 3a–f shows the FESEM images of pure S ­ nO2 and
­V2O5/SnO2 nanocomposite thin films. In the thin films
SV0, SV1, SV2 and SV3 (Fig. 3a–d), it is observed that
the grains are interwoven with each other and form tightly
bound surface and indicates a homogeneous distribution of
grains over the entire surface of the thin films. In sample
SV4 (Fig. 3e), disc-shaped grains are discernible, while in
sample SV5 (Fig. 3f), rhombus-shaped grains are noticed.
Indeed, FESEM images of the thin films SV0, SV1, SV2
and SV3 have grain size in the range ~ 53 to 194 nm. This
indicates that the thin films are composed of both nano and
micro-sized grains. When compared to the samples SV0,
SV1, SV2 and SV3, the micro-sized grains of the samples
SV4 and SV5 are inhomogeneously distributed on the sur-
face of the thin films. Also, the micro-sized grains of the
samples SV4 and SV5 are larger than the samples SV0, SV1,
SV2 and SV3. The growth of these grains is attributed to
the increase of film thickness, which is well supported from
the thickness measurement. Figure 4a–f displays the EDX
spectra of the thin films. Pure ­SnO2 thin film (Fig. 4a) dis-
plays strong binding energy signals near ~ 0.38 keV (Sn), ~
0.34 keV (Sn) and ~ 0.54 keV (O), which reveal the presence
of elements Sn and O. With the addition of ­V2O5 into ­SnO2
thin film (Fig. 4b–f), strong binding energy signals related to
vanadium are also identified near ~ 0.45 keV and 4.95 keV
13

Fig. 2  XRD patterns of the thin
films SV0–SV5
along with the signals of Sn and O. This result further sug-
gests the effective inclusion of V
­ 2O5 into S
­ nO2 matrix and
ascertains the formation of ­V2O5/SnO2 nanocomposite.
3.3 FTIR Analysis
The FTIR spectra of the thin films SV1–SV5 are shown
in Fig. 5. The stretching vibrations identified in the region
400–800 cm−1 can be assigned to Sn–O vibrations of ­SnO2
[28]. The peak located near ~ 635 cm −1 was previously
13
Journal of Materials Science: Materials in Electronics
assigned to Sn–O–Sn stretching mode of surface bridg-
ing oxide. Also the multiple peaks centred in the domain
950–1000 cm −1 were previously assigned to character-
istic ­( V 3+=O, ­V 4+=O and ­V 5+=O) stretching modes of
vanadium [29]. It has been also interpreted that many
metal oxides with more than one oxygen atom bonded
to a single metal atom could also absorb in the domain
970–1020 cm −1 [30]. The other bonds appeared in the
range 1020–2500 cm−1 possibly could correspond to V=O
bonds of the polyvanadate structure consisting of V–O–V
Journal of Materials Science: Materials in Electronics

Fig. 3  FESEM images of the

thin films: a SV0, b SV1, c
SV2, d SV3, e SV4 and f SV5

bridges, V=O stretching and its first overtone, respectively where T is the transmittance and d is the film thickness. The
[31]. thickness of the thin films SV0–SV5 was measured by con-
tact method using a stylus profilometer and they are found
3.4 Optical properties to be 318, 323, 329, 335, 341 and 349 nm, respectively. Also
from the figure, it is observed that the transmittance edge
The transmittance spectra of the thin films SV0–SV5 are red shifted towards longer wavelength region with V ­ 2O 5
shown in Fig. 6a–f. It is clear from the transmittance spectra content and this shift is attributed to the increase in film
that the transparency is changed with the addition of ­V2O5 thickness. The optical absorption spectra of the thin films
into ­SnO2. The absorption coefficient (α) is estimated using characterized by UV–Vis spectrophotometer at room tem-
the relation (Eq. 2) [32]. perature are shown in Fig. 6a–f. From the UV–Vis absorp-
tion spectra, all the thin films exhibited a sharp absorption
ln (1∕T)
𝛼= (2) peak in the UV region (~ 301–350 nm), except SV3. The
d thin films SV0 and SV1 show steep absorption edge below
400 nm, while SV2, SV3 and SV4 display absorption edge

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 Journal of Materials Science: Materials in Electronics

Fig. 4  EDX spectra of the thin films: a SV0, b SV1, c SV2, d SV3, e SV4 and f SV5

13
Journal of Materials Science: Materials in Electronics
Fig. 5  FTIR spectra of the thin
films SV1–SV5
above 400 nm. Indeed, the absorption edges of SV0 and
SV1 are in the UV region due to the interband electronic
transition [33]. Unlike other thin films, SV5 shows a wide
spread absorption edge in the visible region and the steep
edge feature is absent and this feature was previously attrib-
uted to the charge transmission between the binary metal
oxides through interfacial contact [34]. Except SV0, all
other thin films exhibit additional broad absorption peaks
in the visible region (above 400 nm) and these absorption
peaks can be related to the crystal field splitting electronic
transition of vanadium ions in the nanocomposite thin films
[35]. Thus the occurrence of broad absorption peaks in the
visible region clearly indicates the effective inclusion of
­V2O5 in ­SnO2 matrix [36]. Furthermore, with an increase
in ­V2O5 content in the V
­ 2O5/SnO2 thin film, a red shift in
the absorption spectra is noticed. This clearly indicates the
bandgap narrowing feature. The red shift in absorption edge
and bandgap narrowing with an increase in ­V2O5 content
are ascribed to the increase in film thickness. It should be
noted that the thickness of the thin film can cause a change in
band structure due to scattering losses, which in turn could
influence the fundamental absorption edge and bandgap
[37]. The optical absorption is also extended in the visible
regime due to the light absorption characteristics of V­ 2O5. It
is well known that semiconductors can absorb UV–Visible
light below a threshold wavelength λg, the so-called funda-
mental absorption edge [38]. The reported absorption edges
of ­SnO2 and ­V2O5 thin films were at 365 nm (3.40 eV) [39]
and 525 nm (2.36 eV) [40], respectively. Thus the increase
of ­V2O5 content in ­SnO2 could contribute for the extension
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 Journal of Materials Science: Materials in Electronics

Fig. 6  Transmittance and absorbance spectra of the thin films: a SV0, b SV1, c SV2, d SV3, e SV4 and f SV5

13
Journal of Materials Science: Materials in Electronics
of absorption towards visible region as well as the red shift
in the absorption edge. This could be likely due to the shift
in the valance band maxima and conduction band minima
which assist to reduce the bandgap [41]. The optical energy
gap of a semiconductor can be determined using the follow-
ing Tauc’s relation (Eq. 3) [42].
)n
(3)
(
𝛼h𝜈 = k h𝜈 − Eg
where α is the absorption coefficient, K is a constant and
Eg is the energy gap. For allowed direct transition n = 1/2
and for allowed indirect transition n = 2 [43, 44]. ­SnO2 is a
direct bandgap semiconductor (n = 1/2) [45] and thus direct
bandgap of the prepared thin films are calculated. A plot of
(αhυ)2 versus photon energy (hυ) provides the direct band-
gap energy of the semiconductor. A tangent drawn to the plot
intercepts the X-axis and gives a good approximation of the
energy gap of this semiconductor. The bandgap of the thin
films obtained from Tauc’s plot is shown in Fig. 7a–f. From
the figure, it is clear that the bandgap decreases with ­V2O5
content in the ­V2O5/SnO2 nanocomposite thin films. This
could be likely due to the higher carrier density in conduc-
tion and valance bands that leads to energy gap narrowing
as result of high carrier–carrier interaction [46]. The calcu-
lated bandgaps of the thin films SV0–SV5 decrease in the
sequence SV0 = 3.57 eV > SV3 = 3.15 eV > SV1 = 3.12 eV 
> SV2 = 2.96 eV > SV4 = 2.80 eV > SV5 = 2.39 eV. These
results indicate that tuning the concentration of nanocom-
posite thin films may offer a promising route for bandgap
engineering over a wide range of energies [47].
3.5 Gas sensor study
The variation of sensor resistance as a function of time for
SV0 and SV5 thin films is shown in Fig. 8a and b. From the
figure, it is interesting to observe that the transient resistance
of SV5 is lower than SV0 in the recorded time. The modifica-
tion of the overall transient resistance of the composite SV5
could be likely due to the band bending caused by the reaction
of the oxygen ions with the N ­ H3 gas [48]. In a chemiresistive
metal oxide-based sensor, the variation of the sensor signal
could be related to an ionosorption phenomenon and could be
described by the transit of free charge carriers from the metal
oxide sensor layer to the adsorbed surface species (or vice
versa) [48]. It is well known that ­NH3 gas sensing mechanism
of semiconductor-based nanocomposite comprises gas adsorp-
tion, charge transfer and gas desorption [14]. The schematic
illustration for gas sensing mechanism is shown in Fig. 9. The
reactions responsible for the change in transient resistance
after the adsorption of ­NH3 gas is given below [49, 50].
O2(g) + e− → O2(ads) − (4)
4NH3(g) + 3O2(ads) − → 2N2 + 6H2 O + 6e− (5)
Since the gas response is a surface phenomena wherein,
the adsorbed oxygen at grain boundaries traps electrons from
grains of the thin film rather than the glass substrate [51].
Therefore the transfer of electrons is solely due to the grains
available on the surface of the glass substrate. Atmospheric
oxygen present on the surface of the semiconducting thin
film sensor adsorbs electrons from the conduction band,
thereby creating ­O2(ads)− and an electron depletion layer on
the surface of the thin film (Eq. 4). In this study, N ­ H3 gas
gets adsorbed and the conduction band accepts electrons
(Eq. 5) and hence reduces the transient resistance in the
nanocomposite thin film. In addition to this, the decrease
in transient resistance of the ­NH3 adsorbed SV5 sensor
operated at 300 °C is accompanied by two competitive pro-
cesses [14, 50–53]. Firstly, the addition of V ­ 2O5 into ­SnO2
thin film forms weak bonded complex between vanadium
atoms and adsorbed oxygen, leading to an easy dissociation
of weak complex and formation of additional oxygen spe-
cies. This process further activates the reaction between ­NH3
and adsorbed oxygen species, thereby decreasing the resist-
ance of SV5 sensor. Secondly, SV0 thin film showed higher
resistance when compared to SV5 thin film and indicates
that the included ­V2O5 content into ­SnO2 could have formed
new electrical pathways and promoted excellent transfer of
electrons [14]. Therefore, it is imperative to suggest that
decrease of resistance in SV5 thin film has excellent N ­ H3
sensing property than SV0 thin film. Another possible rea-
son for the decrease of resistance in SV5 thin film is due
to its narrow bandgap, increased average crystallite size
and film thickness, as suggested from the UV–Vis, XRD
and thickness measurements, respectively. Furthermore, to
exploit the prepared material effectively for sensing applica-
tion, sensor parameters (sensor response, response time and
recovery time) have to be measured. The sensor response (S)
is calculated using the relation (Eq. 6) [22].
Ra
S=
Rg (6)
where Ra and Rg are the electrical resistances of the sensor
in air and ­NH3 gas, respectively. Since there is a fluctuation
in baseline parameters (resistance and time), sensor param-
eters are measured for the sensor signal located between the
time window 400 and 650 s. Fluctuations in sensor signals
of SV5 thin film are also controlled significantly with the
addition of ­V2O5 content to pure ­SnO2. The measured sen-
sor response, response time and recovery times for SV0 thin
film are 92.34, 30 and 44 s, while they are 99.13, 39 and
180 s for SV5 thin film. Although the response and recovery
times of SV5 are higher than SV0, its higher sensor response
is highly desirable for N­ H3 sensing application. Also, the
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 Journal of Materials Science: Materials in Electronics

Fig. 7  Tauc’s plot diagram of the thin films: a SV0, b SV1, c SV2, d SV3, e SV4 and f SV5

13
Journal of Materials Science: Materials in Electronics

Fig. 8  Transient resistance vs. time graphs of the thin films: a SV0 and b SV5

Fig. 9  Schematic illustration
representing the gas sensing
mechanism of the thin film SV5
exposed to air and ­NH3 gas

obtained sensor response of SV5 thin film (~ 99.13) is higher
than materials such as ­SnO2/MWCNT (~ 28) and Pd/SnO2/
RGO (~ 19.6), while the response and recovery times (~ 39
and 180 s ) are faster than ­SnO2/MNCNT (~ 593 and 854 s )
and Pd/SnO2/RGO (~ 50 min and ~ 50 min ) [13, 14]. These
results further indicate that the prepared SV5 thin film is a
promising candidate for ­NH3 sensing application in the field
of environmental measurement and control.

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 Journal of Materials Science: Materials in Electronics

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